CN102491880B - Technique for extracting resveratrol and pigment from grape skin - Google Patents
Technique for extracting resveratrol and pigment from grape skin Download PDFInfo
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- CN102491880B CN102491880B CN201110384512.9A CN201110384512A CN102491880B CN 102491880 B CN102491880 B CN 102491880B CN 201110384512 A CN201110384512 A CN 201110384512A CN 102491880 B CN102491880 B CN 102491880B
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Abstract
The invention relates to a technique for extracting effective ingredients from a natural product, particularly a technique for extracting resveratrol and pigment from grape skin, which comprises the following steps: drying the grape skin, pulverizing, extracting resveratrol by ultrasonic waves, extracting pigment by ultrasonic waves, and purifying to obtain the resveratrol product and the pigment product. In the technical scheme provided by the invention, double solvents and ultrasonic extraction are integrated; the technical scheme provided by the invention has the advantages of high extraction efficiency, low extraction cost and low energy consumption by using the ultrasonic extraction technique according to the principle that the resveratrol and pigment in the grape skin have different solubilities in solvents with different polarities; the solvents used in the extraction process can be utilized cyclically, so that the solvent consumption is low, and the environmental influence is low, thereby avoiding destroying the bioactivities of the resveratrol and the pigment in the extraction process; and thus, the invention is suitable for extracting bioactive substances.
Description
Affiliated technical field
The present invention relates to a kind of from natural product the technique, particularly a kind of technique of extracting trans-resveratrol and pigment from Pericarpium Vitis viniferae of extracting effective components.
Background technology
The effects such as that trans-resveratrol has is anti-oxidant, anti-ageing, anticancer, reducing blood-fat, beauty treatment, fat-reducing; Grape skin color is natural pigment, can be widely used in the food service industrys such as jam, fruit wine, compares with synthetic colour, has certain nutritive value and pharmacological action; According to related data statistics, trans-resveratrol and grape skin color are very well sold and in short supply in world market, are in great demand, and have that prospect of very wide market.Due to the pigment containing in Pericarpium Vitis viniferae, poor, unstable, the easy inactivation of its high thermal resistance of trans-resveratrol, must under comparatively gentle condition, extract.
Due to the growth of output vinous, how the Pericarpium Vitis viniferae that rear generation is a large amount of, effectively utilize trans-resveratrol and pigment in Pericarpium Vitis viniferae at present, and the pressure that reduces environment becomes one of focus of people's research.The method that present stage is extracted trans-resveratrol or pigment from Pericarpium Vitis viniferae mainly contains solvent-extraction process, supercritical CO
2extraction method, microwave extraction method etc., in aforesaid method, the main problem existing is as follows: 1, solvent-extraction process mainly exists organic solvent consumption many, extraction process length consuming time, production cost is high, in the product obtaining, remains solvent, and in the process of extracting, solvent leaks simultaneously, cause the problems such as extraction environment is poor, environmental pollution, if control solvent, leak, certainly will cause production unit complexity, investment and process cost high, the series of problems such as cost increase; 2, supercritical CO
2extraction method is mainly that production cost is too high, higher to the requirement of operational condition; 3, the weak point of microwave extraction method existence is, the selection of spe medium is larger to product components influence, causes the loss of part effective constituent.
In the trans-resveratrol or pigment process of aforesaid method in extracting Pericarpium Vitis viniferae, also have that extraction yield is low, the high problems that consume energy, and just extracted trans-resveratrol or a kind of material of pigment in Pericarpium Vitis viniferae.
Summary of the invention
The object of the invention is to solve the defect that prior art exists, provide a kind of extraction yield high, consume energy lowly and little to environmental hazard, can from Pericarpium Vitis viniferae, extract the technique of trans-resveratrol and pigment simultaneously.
Technical scheme of the present invention is: a kind of technique of extracting trans-resveratrol and pigment from Pericarpium Vitis viniferae, and its processing step is:
1) Pericarpium Vitis viniferae is dry: by the grape skin reclaiming after wine liquid, remove residual moisture to water ratio be less than 4% through natural air drying;
2) pulverize: the Pericarpium Vitis viniferae after air-dry is crushed to after 60-80 order stand-by;
3) ultrasonic extraction trans-resveratrol: the Pericarpium Vitis viniferae after pulverizing is put into weak polar solvent, adopt ultrasonic extraction, wherein the weight of Pericarpium Vitis viniferae and weak polar solvent, volume ratio are 1: 2.5～15, extract 20～50 ℃ of temperature, extraction time 10～20min, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and is reclaimed solvent, utilize recovered solvent again to extract filter residue, extract temperature and time with extract for the first time identical, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and reclaim solvent; After the concentrated solution of extracted twice is mixed, after being dried, obtain trans-resveratrol meal, after trans-resveratrol meal is purified, obtain trans-resveratrol product;
4) ultrasonic extraction pigment: the filter residue after said extracted trans-resveratrol is put into the solvent that polarity is stronger, adjust pH value to 3 left and right of solution, then adopt ultrasonic extraction; The weight of the solvent that wherein filter residue and polarity are stronger, volume ratio are 1: 5～15, extract 10～60 ℃ of temperature, extraction time 5～11min, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and reclaims solvent, utilize recovered solvent again to extract filter residue, extract temperature and time and extract for the first time identically, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and reclaims solvent, after the concentrated solution of extracted twice is mixed, after dry pigment meal, after purified pigment product.
Above-mentioned weak polar solvent is chloroform, acetone, ether, ethyl acetate.
The solvent that above-mentioned polarity is stronger is methyl alcohol, water, ethanol, Virahol.
Above-mentioned dry employing vacuum-drying, drying temperature is 40-60 ℃.
The purifying of above-mentioned trans-resveratrol meal is to adopt macroporous resin to carry out Static Adsorption and wash-out, to remove the partial impurities such as polysaccharide, and the further separation and purification of recycle silicon plastic column chromatography.
The purifying of above-mentioned pigment meal is to adopt silica gel column chromatography to carry out separation and purification to extracted pigment.
Technical scheme employing solvent pairs of the present invention and supersound extraction are integrated, different with the solvability of pigment in the solvent of opposed polarity according to trans-resveratrol in Pericarpium Vitis viniferae, utilize the special roles such as judder that ultrasonic wave produces, very high acceleration, strong cavitation effect, stirring, improve the impact velocity between material molecule, make technical scheme of the present invention there is following characteristics: 1, extraction efficiency is high, extraction cost is low.Adopt ultrasonic wave extraction, promoted trans-resveratrol, pigment to the dissolution rate of extracting in solvent, thereby greatly reduced the consumption of solvent, reduced extraction cost, improved extraction efficiency, for suitability for industrialized production is laid a good foundation.Compared with prior art, the extraction yield of trans-resveratrol can improve doubly left and right of 1.4-4, extracts temperature and reduces half left and right, and the extraction yield of pigment can improve nearly one times, extract temperature and reduce half left and right, the purity of trans-resveratrol and pigment finished product has compared with prior art improved 10-15 percentage point; 2, the processing condition that the present invention extracts are gentle, avoided the bioactive destruction of in leaching process trans-resveratrol and pigment, are applicable to having the extraction of biologically active substance.3, energy consumption of the present invention is low.Because extraction time is short, extract the features such as temperature is low, solvent load is few, reduced energy consumption, reduced the discharge of refuse.4, due to solvent used in leaching process can recycle, solvent load is little, lower on the impact of environment.
The present invention contrasts as following table with pigment index with the trans-resveratrol that prior art is produced:
Accompanying drawing explanation
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
The process flow sheet that extracts grease and pycnogenols from Semen Vitis viniferae as shown in Figure 1, embodiment is as follows.
Embodiment 1:
1) grape skin is dry: by the grape skin reclaiming after wine liquid, through natural air drying remove residual moisture to water ratio in 3% left and right.
2) pulverize: the Pericarpium Vitis viniferae after air-dry is crushed to after 80 orders stand-by.
3) ultrasonic extraction trans-resveratrol: take and pulverize rear 80 object Pericarpium Vitis viniferae 2g, the ethyl acetate 14ml that adds volume fraction >=99.5%, being placed in supersound extraction device extracts, extracting temperature is 40 ℃, extraction time 15min, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and is reclaimed solvent, utilize recovered solvent again to extract filter residue, extract temperature and time with extract for the first time identical, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and reclaim solvent; After the concentrated solution of extracted twice is mixed, be placed in the vacuum drying oven of 40 ℃, after being dried, obtain trans-resveratrol meal.The extraction yield of trans-resveratrol is 1.2%.
4) ultrasonic extraction pigment: take the filter residue 2g after said extracted trans-resveratrol, adding 10ml volume fraction is 60% ethanolic soln, and to utilize volume fraction be that the pH value that 0.3% HCl solution is adjusted above-mentioned solution is 3, then being placed in supersound extraction device extracts, extract temperature 60 C, extraction time 9min, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and is reclaimed solvent, utilize recovered solvent again to extract filter residue, extract temperature and time with extract for the first time identical, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and reclaims solvent, the concentrated solution merging of extracted twice is placed in vacuum drying oven and is dried, 60 ℃ of drying temperatures, dry rear gained pigment meal, with this understanding, the extraction yield of pigment is 22.9%.
5) purifying of trans-resveratrol: take NKA-9 type macroporous resin 1g that pre-treatment is good in the tool plug Erlenmeyer flask of 50ml, and the trans-resveratrol meal 0.5g that takes dry gained to be dissolved in 10ml volume fraction be in 70% ethanolic soln, join in tool plug Erlenmeyer flask and be placed on shaking table and vibrate, vibration temperature is 30 ℃, adsorption time 15min; After absorption, the first water of saturated polymeric adsorbent is carried out to wash-out, until elutriant is water white transparency, object is to remove the impurity such as inorganic salt, polysaccharide, protein, the ethanolic soln that is 80% by 100ml volume fraction again carries out wash-out again, and elution time is 40 ℃ of 15min, eluting temperatures.Solvent, the concentrated a small amount of liquid that contains trans-resveratrol of obtaining are collected, reclaimed to elutriant.Further by silica gel column chromatography, carry out separating-purifying, the volume proportion of elutriant is the sherwood oil of 1: 1: acetone mixing solutions carries out gradient elution, to elutriant Fractional Collections, concentrated, and reclaims solvent, vacuum-drying obtains more pure white veratryl alcohol powder, and purity reaches more than 95%.
6) purifying of pigment: first use sherwood oil: the mixed solution that the volume ratio of ethanol is 1: 1 carries out wash-out, remove a part of yellowish green flavonoid material, again with ethanol, carry out wash-out, collect, concentrate wine-colored liquid, reclaim solvent simultaneously, dry under vacuum condition, obtain purer Pericarpium Vitis viniferae cyanidin(e) powder, purity reaches more than 95%.
As the case may be, in above-mentioned ultrasonic extraction pigment processing step, the adjustment of pH value can adopt other acidic solution to carry out, and its objective is that the pH value of adjusting solution is for acid.
Embodiment 2-3:
The extraction of trans-resveratrol: on the basis of case study on implementation 1, change to extract temperature (℃), extraction time (min), extraction time, solid-liquid ratio (g/ml), granular size etc. processing parameter, specifically implement parameter as shown in the table:
The purifying parameter of trans-resveratrol is: change resin model, loading concentration, vibration temperature ℃, adsorption time, elution concentration, elution time min, eluting temperature ℃, as following table:
In above-described embodiment 2-3, utilize extracting the parameter that filter residue after trans-resveratrol extracts pigment is: volume fraction of ethanol, extract temperature (℃), extraction time (min), extraction time, solid-liquid ratio (g/ml), specifically implement parameter as shown in the table:
| Embodiment | Ethanol | PH value | Temperature | Number of times | Solid-liquid ratio | Extraction time | Extraction yield (%) | Purity |
| 2 | 50％ | 2 | 50℃ | 2 | 1∶5 | 5 | 20.67％ | 93.5％ |
| 3 | 70％ | 4 | 70℃ | 3 | 1∶9 | 15 | 21.38％ | 94.7％ |
Embodiment 4-7:
The extraction of trans-resveratrol: on the basis of case study on implementation 2-3, other extraction conditions immobilize, only changes and extracts solvent, specifically implements parameter as following table:
The extraction of pigment: on the basis of case study on implementation 2-3, other extraction conditions immobilize, only changes the volume fraction of extracting solvent, specifically implements parameter as following table:
In above-described embodiment 2-7, the purifying of pigment is identical with embodiment 1.
Claims (2)
1. from Pericarpium Vitis viniferae, extract a technique for trans-resveratrol and pigment, its processing step is:
1) Pericarpium Vitis viniferae is dry: by the grape skin reclaiming after wine liquid, remove residual moisture to water ratio be less than 4% through natural air drying;
2) pulverize: the Pericarpium Vitis viniferae after air-dry is crushed to after 60-80 orders stand-by;
3) ultrasonic extraction trans-resveratrol: the Pericarpium Vitis viniferae after pulverizing is put into weak polar solvent, adopt ultrasonic extraction, wherein the weight of Pericarpium Vitis viniferae and weak polar solvent, volume ratio are 1:6-8, and above-mentioned weak polar solvent is chloroform, ether; Extract 20～30 ℃ of temperature, extraction time 10～20min, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and reclaimed solvent, utilize recovered solvent again to extract filter residue, extract temperature and time with extract for the first time identical, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and reclaim solvent; After the concentrated solution of extracted twice is mixed, after being dried, obtain trans-resveratrol meal, trans-resveratrol meal carries out Static Adsorption and wash-out through macroporous resin, to remove polysaccharide partial impurities, after the further separation and purification of recycle silicon plastic column chromatography, obtains trans-resveratrol product;
4) ultrasonic extraction pigment: the filter residue after said extracted trans-resveratrol is put into the solvent that polarity is stronger, adjust pH value to 2-4 of solution, then adopt ultrasonic extraction; The weight of the solvent that wherein filter residue and polarity are stronger, volume ratio are 1:5～9, and the solvent that above-mentioned polarity is stronger is water, Virahol; Extract 10～60 ℃ of temperature, extraction time 5～11min, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and reclaim solvent, utilize recovered solvent again to extract filter residue, extract temperature and time with extract for the first time identical, after extraction finishes, extracting solution is filtered to get filtrate and filter residue, filtrate is concentrated and reclaim solvent; After the concentrated solution of extracted twice is mixed, after being dried, obtain pigment meal, pigment meal carries out separation and purification through silica gel column chromatography, obtains pigment product after purifying.
2. the technique of extracting trans-resveratrol and pigment from Pericarpium Vitis viniferae according to claim 1, is characterized in that above-mentioned dry employing vacuum-drying, and drying temperature is 40-60 ℃.
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| CN103103063B (en) * | 2013-01-29 | 2015-02-18 | 新疆西部牧业股份有限公司 | Technology for producing distilled wine by use of grape skin residue |
| CN104435405B (en) * | 2014-11-22 | 2018-05-29 | 浙江大学 | Natural plant extracts and the purposes for preventing Nosema apis parasitosis |
| CN105440732B (en) * | 2015-11-06 | 2017-08-29 | 大兴安岭林格贝寒带生物科技股份有限公司 | The method of enriching and purifying rouge radish anthocyanidin |
| CN105384605A (en) * | 2015-12-09 | 2016-03-09 | 重庆三零三科技有限公司 | Technology for extracting resveratrol from grape leaf |
| CN106242953A (en) * | 2016-07-14 | 2016-12-21 | 中国林业科学研究院林产化学工业研究所 | A kind of method preparing resveratrol from phoenix seed of Flos Moutan shell |
| CN106387910A (en) * | 2016-09-05 | 2017-02-15 | 广西大学 | Preparation method of nephelium lappaceum shell extract |
| CN106634028A (en) * | 2016-12-09 | 2017-05-10 | 新疆维吾尔自治区产品质量监督检验研究院 | High-efficiency grape skin pigment extraction process |
| CN111925883A (en) * | 2020-08-27 | 2020-11-13 | 郭占伟 | Peach red wine rich in resveratrol and preparation method thereof |
| CN115636734A (en) * | 2022-10-18 | 2023-01-24 | 西夫拉姆酒业集团有限公司 | Resveratrol purification process for red wine |
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Effective date of registration: 20160325 Address after: 733006 Gansu province Wuwei city Liangzhou District huangyangzhen Nongda Road No. 9 Patentee after: GANSU SHOULUSHAN PHARMACEUTICAL CO., LTD. Address before: 622 box 539, Ningxia University, 750021 Shanxi Road, Yinchuan, the Ningxia Hui Autonomous Region, Helan Patentee before: Ningxia Univ |